反应详情

A solution of 80 (0.2 g, 1.0 mmol) and 81 (0.2 g, 1.17 mmol) in toluene (5 mL) was heated at reflux for 4 hours. The reaction was cooled and mixed with 0.5 N NaOH (5 mL), then extracted with ethyl acetate (2×10 mL). The organic material was combined, dried (K2CO3) then concentrated under reduced pressure. The residue was purified by flash chromatography (SiO2, gradient elution, hexane to 3:1 hexane/ethyl acetate) to give 82 (228 mg, 68%) as a yellow oil.

1. temperatureat reflux for 4 hours
2. temperatureThe reaction was cooled
3. extractionextracted with ethyl acetate (2×10 mL)
4. dry with materialdried (K2CO3)
5. concentrationthen concentrated under reduced pressure
6. customThe residue was purified by flash chromatography (SiO2, gradient elution, hexane to 3:1 hexane/ethyl acetate)